Isopropylamine → HCID 3550524, compound

HRID 652295Notes

Reaction equation

HRID 652295 reaction equation
[Cl:1][CH:2]([Cl:6])[C:3](Cl)=[O:4].[CH:7]([NH2:10])([CH3:9])[CH3:8]>C(Cl)Cl>[CH:7]([NH:10][C:3](=[O:4])[CH:2]([Cl:6])[Cl:1])([CH3:9])[CH3:8]

Participants

4

Conditions

Temperature
0 °C

Procedure

Dichloroacetyl chloride, 442.5 grams (3.0 mole), was dissolved in a flask containing 900 milliliters of methylene chloride and the solution cooled to 0° C. in an ice/acetone bath. 354 grams (5.98 mole) of isopropyl amine was added dropwise with vigorous stirring and the addition rate was adjusted to maintain the reaction temperature below 5° C. When the addition was complete, the mixture was allowed to stir at ambient temperature for one hour then washed with 2×500 milliliters water, the organic phase separated, dried over magnesium sulfate and stripped of solvent at reduced pressure giving 499 grams (98% yield) of the desired product, a white solid, m.p. 45°-48° C.

Workup

  1. temperatureto maintain the reaction temperature below 5° C
  2. additionWhen the addition
  3. stirringto stir at ambient temperature for one hour
  4. washthen washed with 2×500 milliliters water
  5. customthe organic phase separated
  6. dry with materialdried over magnesium sulfate

Sources & evidence

ORD record
ord-3891246f27e4482a92d8af954f01cd03
Source dataset
uspto-grants-1987_06
Patent number
US04670593

Reaction notes

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